83Estimation of Ferrite Grain Size and... 2018 62 1

Estimation of Ferrite Grain Size and Mechanical Properties of a 22MnVNb6 Microalloyed Low Carbon Cast Steel

Ganwarich Pluphrach1*, Somchai Yamsai1

Received 07 September 2017; accepted after revision 18 September 2017

AbstractThe ferrite grain size of a 22MnVNb6 microalloyed steel can be estimated by developing a relationship between ferrite grain size, austenitising temperature and cooling rate from austeni-tising time, temperature. An extended Hall-Petch relationship was used to estimate the yield stress from the estimation fer-rite grain size. Heat treatment as the annealing was used to improve the tensile and hardness properties of the steel. It was shown that the best combination of tensile and hardness prop-erties were achieved when a higher austenitising temperature was used. Transmission electron and optical microscopy were used to study the morphology of ferrite and pearlite formed by the heat treatments. The microstructural studies showed that partition of grain by as-cast state was probably the reason for austenite and ferrite grain size improvement. Considering the experimental results, maximum errors of 14.5% and 7.5% were found in the estimation of ferrite grain size and tensile strength, respectively.

Keywordsgrain size, mechanical properties, Microalloyed Steel, Hall-Petch relationship

1 IntroductionThe name “Microalloyed Steels” was first applied to a class

of higher strength low carbon containing small additions of niobium and/ or vanadium. Any attempt at a rational definition of microalloying based on the increases in strength produced by small additions would now include aluminium, vanadium, titanium and of course niobium-treated steels. The effects of the microalloying elements are also strongly influenced by ther-mal treatments [1, 2]. The transformation product grain size control is an important parameter in thermal and mechanical processing of microalloyed steels. It has been well recognized that the tensile and hardness properties of steels are strongly related to the microstructure, specially the grain size [3, 4]. In the heat treatment of microalloyed low carbon cast steels involving the austenitising and cooling treatments, the parame-ters such as cooling rate and austenitising temperature and time have considerable influence on the ferrite grain size and tensile and hardness properties of the steels. It has been shown that accelerated cooling treatment refines the ferrite grain size while increasing the austenitising time and temperature increases the ferrite grain size. Several studies on accelerated cooling have been carried out, considering the relation of processing parameters and tensile and hardness properties to the micro-structures [5]. In those studies the relationships presented for estimating ferrite grain size were deduced experimentally to ralate the ferrite grain size to the cooling rate and prior austen-ite grain size [6-9]. The grain size estimation model presented by Umemoto et al., is extended in this research to develop a relationship between ferrite grain size, cooling rate, austeniting time, and temperature. The following Hall-Petch relationship is utilized to relate the yield stress to the ferrite grain size [10-14]

σ σ αy Kd= + −0

0 5.

where σy is the yield stress, σo and K are constants, dα the fer-rite grain size. The grain size of a microalloyed steel has an important effect on its properties. This phenomenon is known in the literature as the grain size effect. As far as the tensile and hardness properties of the steel is concerned (such as yield and flow stress, ductility, hardness and fatigue limit), a refinement

1 Department of Mechanical Engineering, Faculty of Engineering, Srinakharinwirot University, Ongkharak, Nakhon-nayok, 26120, Thailand* Corresponding author, e-mail: pganwarich@yahoo.com

62(1), pp. 83-89, 2018https://doi.org/10.3311/PPme.11458

Creative Commons Attribution b

research article

PPPeriodica Polytechnica Mechanical Engineering

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84 Period. Polytech. Mech. Eng. G. Pluphrach, S.Yamsai

of the grain size generally results in an improvement of these properties at low temperature. Since the grain boundaries are known to block the movement of crystal dislocations, the grain size effect has been explained in term of the distance a disloca-tion can slip. The improved yield strength can be attained only by carefully controlled heat treatment. Normalizing and/or solution annealing come under consideration. Yield strength of microalloyed metallic material obeys extended Hall-Petch relationship [15, 16] as follows

R R R R R Ry o a g p t= + + + +∆ ∆ ∆ ∆

Where Ro is friction stress, DRa is related to solid solution strengthening being linearly proportional to the concentration of alloying elements, DRg is a grain size contribution, DRp is precipitation strengthening and is the proportional to precip-itation potential, DRt is matrix phase transformation strength.

1.1 Determination of austenite grain size distributionAustenite grain size distribution can be recorded by pho-

tographing the microscopic picture and the determination requires measurement of each individual grain. Austenite grain size distribution in one dimension is the distribution of the lengths of linear intercepts through the grains. Metallographic techniques for measuring austenite grain size were originally base on point counting or linear intersection lengths (chords) distrbutions, the derivation by Spektor appears to be the first [17, 18]. The working formula is obtained [12] as below

N jn j

j

n j

jvL L

( )( ) ( )

=−

−+

+

4

2 1

1

2 12π∆

Where N jν ( ) is the number of particles of mean diameter per unit volume in the interval 2 1 1j n jL− +( ), is the number of chords per unit length of test line. The austenite grain size micro-structures of entire the relevant samples representative photomi-crographs were taken. In order to determine the austenite grain size, the samples were specially etched in a saturated piric acid solution at about 80°C [19, 20]. The austenite grain size was then measured at magnification 25× using a filler eyepiece. The degree of magnification will be limited by the fact that the picture must include a sufficient number of grain [21-23].

1.2 Estimation of Ferrite Grain SizeWhen ferrite nucleation occurs homogeneously in the austen-

ite matrix, ferrite grain is independent of austenite grain size. In the case that ferrite nucleation occurs at austenite grain corners, ferrite grain size is proportional to dg . The ferrite grain size is determined by the number of ferrite nucleations at austenite grain surfaces until these surfaces are completely occupied by ferrite grains. During cooling, ferrite grains are nucleated and grown at each temperature with corresponding nucleation and growth rates. On the temperature Ti ferrite nucleates at the rate

Is (Ti ) and grows at the rate α (Ti ), where Is (Ti ) and α (Ti ) are the nucleation rate and the parabolic rate constant in the isothemal transformation at temperature Ti [24]. Ferrite grains number na nucleated at temperature Ta during cooling was cal-culated by Umemoto et al. [25] as

n I T dtI T

Q TdTa s a a

s a

a

= =

( )

( )

( )

where Q T dT dta( ) = − is the cooling rate. Assuming that, fer-rite nucleation occurs at nα is proportional to CRn1 , where CR and n1 are the cooling rate. If ferrite nucleation occurs at aus-tenite grain edges & corners, nα is proportional to CRn2 and CRn3 . Ferrite grain size can be calculated as follows [25, 26]

dS ngb

αα

=

2

3

1

3

where Sgb is the austenite grain surface area per unit volume.As increasing the austenite grain size and decreasing the

cooling rate, ferrite grain size is increased. Determining the prior austenite grain size in heat treatment of microalloyed steels, one may substitute by the austenitising time t and tem-perature T as below [7, 27]

d k tQRT

kγ =

−

1

2exp

where positive constants are k1, k2, & Q. Therefore, the ferrite grain size is derived from Eq. (10) and (9) as follows

d aAT

CR tn m

α =−

( )− exp

where positive constants are a, A, n, & m. Using this equation and measuring the austenitising time, temperature, and cool-ing rate, the ferrite grain size of the 22MnVNb6 Microalloyed Steel can be estimated. The estimated ferrite grain size and the Hall–Petch relationship from Eq. (1) determine the yield strength of this steel.

2 Experimental ProcedureWith different austenitising times, temperatures, and cooling

rates from the tests of heat treatment were carried out to deter-mine of values a, A, n, & m from Eq. (7). A commercial strip of 22MnVNb6 microalloyed low carbon cast steel 30.00 mm long, with a rectangular cross section, 20.00 mm wide by 5.00 mm thick was applied on the tests [28-31]. The research material having chemical composition showed in Table 1. Surface pro-cessing operations for property enhancing to determine the dα , the test of heat treatment programmes are showed in Table 2 and have been utilized. Using thermocouple to determine the cooling rate of each specimen, it was utilized to record the data of temperature at austenitising time 1 s. Transmission electron

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85Estimation of Ferrite Grain Size and... 2018 62 1

microscopy (TEM) was the most widely used technique for studying all aspects of phase transformations in steels over the length scale range 1–100 nm [32]. TEM data was used as a start-ing point for the proposed model in micromagnetic simulation for electrodeposited nickel nanowires [33]. Defects created by the superelastic cycling in thin Ni–Ti wires were analyzed by TEM [34]. TEM studies were carried out on the some samples of the as-cast state and the heat treatment test. Optical microscopy was used to examine the microstructure of the microalloyed steel specimen in as-cast state and the heat treatment test. In order to determine the microstructure, the samples are specially etched in 5% nital solution [9]. The concentration of the nital solution has to be adjusted for different samples. The microstructure is then measured at magnification 50x using a filler eyepiece. It was observed that the microstructures consisted of ferrite and a small amount of pearlite. The classic data in the literature for the grain size dependence of the strength in many metals are reviewed [13]. The ferrite microstructure determination should be done in a magnification suited to the size of the grain so that small grains may not be lost. The degree of magnification will be limited by the fact that the picture must include sufficient ferrite grain size. The ferrite grain size of each specimen was measured according to ISO 643 standard. To determine yield strength of the as–cast state steel of a 22MnVNb6 microalloyed, the different ferrite grain size microstructures of the steel were determined and calculated by using the Spektor equation and extended Hall-Petch relationship. After calculating a, A, n, and m in Eq. (7) and the extended Hall-Petch relationships for the low carbon microalloyed steel, some heat treatment as the annealing was carried out in order to compare estimated ferrite grain size and strength data.

3 Result and DiscussionThe annealing was already used to improve the tensile and

hardness properties of the 22MnVNb6 microalloyed low carbon cast steel in as-cast state. Since the austenite and ferrite grain size of microalloyed steel are important factor, they were necessary to show the grain size with austenite and ferrite as in Fig. 1 and ferrite-pearlite micrograph of heat treated as annealing in Fig. 2. The microstructures were examined using light microscopy and by transmission electron microscopy of thin foils. Representa-tive TEM images of a 22MnVNb6 microalloyed steel are given on as-cast state in Fig. 3 and on the austenitising temperature at 1000 °C in Fig. 4 [35, 36]. The austenite grain size of the as-cast microalloyed steels were investigated using Spektor’s analysis in order to determine the size distribution. The prior austenite grain boundaries were revealed by etching the specimens for evaluated the mean grain size. Table 3 shows size distribution of austenite grain and Table 4, there is comparison between the mean austenite grain size of Spektor’s method and the values of G, đ & l of International standard [10, 37-40]. The microal-loyed steel was studied investigated to optimize the influence of single and multiple microalloying additions on the ferrite grain size microstructure in as-cast state. Ferrite grain size distribu-tions can be recorded by photographing the microscopic picture and the determination requires measurement of each individual grain. Ferrite grain size distribution in one dimension is the dis-tribution of the lengths of linear intercepts through the grains. Metallographic techniques for measuring ferrite grain size were originally based on point counting or linear intersection length distribution. The ferrite grain size of microalloyed steel is important factors, on Table 5 shows size distribution and grain size contribution to yield stress. Table 6 shows estimation of

Table 1 Chemical composition of a 22MnVNb6 Microalloyed Steel in As-Cast State used in this research work, wt-%

C Mn Si P S Cu Ni V Ti Nb Al N

0.22 1.39 0.38 0.017 0.017 0.22 0.16 0.09 0.01 0.05 0.079 0.017

Table 2 The test of heat treatment programmes used in this research study (using Eq. (8) to determine the dα )

Austenitising temperature,°C Austenitising time, (s) Cooling rate, °C/s dα (μm)

900

660 60,40,12,6.3,5 15.8,17.0,21.4,24.2,25.3

840 60,40,12,6.3,5 17.2,18.6,23.4,26.4,27.6

1020 60,40,12,6.3,5 18.5,20.0,25.1,28.4,29.7

1230 60,40,12,6.3,5 19.8,21.4,26.9,30.4,31.8

1000

680 60,35,15,9,7 22.7,25.2,29.6,32.6,34.2

860 60,35,15,9,7 24.8,27.4,32.2,35.5,37.3

1040 60,35,15,9,7 26.6,29.4,34.6,38.1,40.0

1220 60,35,15,9,7 28.2,31.2,36.7,40.4,42.4

Table 3 Size distribution of austenite grain of microalloyed steel in as-cast state

SteelRange of chord lengths, μm

Number of chords per mm, NL(j)

Diameter of grains, mm, dj

Number of grains per mm3, Nv(j)

Evaluated mean grain size, μm, đ

22MnVNb6 0-170 231 0.017-0.170 1.5417×105 36.1

86 Period. Polytech. Mech. Eng. G. Pluphrach, S.Yamsai

Fig. 1 On the left, austenite grain size microstructure of the steel 22MnVNb6 in as-cast state, as 100 μm , on the right, ferrite grain size microstructure of the same steel as 100 μm , using 2 magnifications according to show some importance of pearlite

Fig. 2 The 100 μm ( ) ferrite-pearlite micrograph of heat treated as annealing samples of steel 22MnVNb6, 900°C (left), and 1000°C (right)

Fig. 3 On the TEM, foil, BF as 0.2 μm , the left as ferrite microstructure of steel 22MnVNb6 and the right as interface between ferrite and pearlite of the same steel

Table 4 Comparison of austenite mean grain size determined by Spektor’s method with estimated austenite grain characteristics according to International standard (ISO643)

SteelEvaluated mean grain size, μm, đ

Estimated grain size (Index), G

Mean diameter of grain, μm,đ

Mean intersected segment, μm,l

22MnVNb6 36.1 6.5 37.7 34.2

87Estimation of Ferrite Grain Size and... 2018 62 1

yield strength of microalloyed steel on the test of heat treatment programmes, based on extended Hall-Petch relationship, with comparative mechanical properties addition. To determine the a, A, n, and m values in Eq. (8) for the test microalloyed steel, graphs of dα versus t for different austenitising temperature and cooling rates were plotted, as presented in Fig. 4 and 5. It is interesting to note that, as these figures show, the experimental relationships between dα , t, and CR are linear. This is accor-dance with Eq. (8). Referring to graphs of dα versus t the ferrite grain size can be expressed as

dT

CR tα =−

( )−18152

10174 0 19 0 37exp

. .

Where dα , CR, t, and T are expressed in μm, °C/s, s, and K, respectively.

Considering the experimental results showed in Fig. 4 and 5 and Eq. (8), by increasing the austenitising time and tem-perature and decreasing the cooling rate, the ferrite grain size transforming from austenite is increased. In fact, by increas-ing the austenitising time and temperature, the prior austenite grain size is increased, and nucleation sites for ferrite forma-tion are decreased. Atom possessing an energy level of the reactants and activation energy will have sufficient energy to react spontaneously to reach the reacted state of energy of the products [41]. A basic procedure for determining the activa-tion energy was developed by Conrad and Wiedersich [42]. By decreasing the cooling rate, the activation energy for nucle-ation is decreased and a smaller number of ferrite nucleation sites produce large ferrite grain size.

4 ConclusionsThe Hall-Petch relationship can be utilized to examine the

dependence of yield stress on ferrite grain size of the as-cast state steel, but extended Hall-Petch relationship can be utilized of the betterment that on the test of heat treatment programmes. When increased by the austenitising temperature, the effects

Table 5 Size distribution of ferrite grains and grain size contribution to yield stress of microalloyed steel in as-cast state

SteelRange of chordlengths, μm

Number of chordsper mm, NL(j)

Diameter of grains, mm, dj

Number of grainsper mm3, Nv(j)

Evaluated mean grain size, μm,đ

Kdα−0.5

(MPa)

22MnVNb6 0-130 625 0.013 -0.130 14.0886×105 20.2 140.8

Table 6 Estimation of yield strength of microalloyed steel on the test of heat treatment programmes, based on extended Hall-Petch relationship, with comparative mechanical properties addition

Microalloyed Steel Heat Temp. (°C) Ro DRa DRg DRp DRt Ry (MPa) Vickers Hardness (HV10) Tensile Strength (σu:MPa)

22MnVNb6900 40 121 169 21 73 424 186 639

1000 40 121 143 38 98 440 187 651

Fig. 4 (Left) According to the X 20 k precipitates of ferrite grain size of the steel 22MnVNb6, (right) using the diffraction pattern TEM replica, SAD, for austenitising temperature at the 1000 °C to find those precipitates of the steel

Fig. 5 Graph of ferrite grain size on cooling rate using austenitising temperature 900°C, as shown orange graph of austenitising time 1230 (s),

blue graph of 1020 (s), red graph of 840 (s), and azure graph of 660 (s)

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88 Period. Polytech. Mech. Eng. G. Pluphrach, S.Yamsai

of austenitising time and cooling rate on ferrite grain size are decreased. When dα formed by continuous cooling transforma-tion, is decreased with an increase in cooling rate or decrease in austenitising time and temperature, the dα can be shown as in Eq. (8). Also, it’s good correlation between experimental and estimated ferrite grain size, yield stress of the material studied of this research work.

AcknowledgementsThe authors would like to express their gratitude to K.

Macek, Faculty of Mechanical Engineering, Czech Technical University in Prague, Czech Republic, for his help with some experiments, discussions, the Strategic Wisdom and Research Institute, Srinakharinwirot University and the Srinakharinwirot University, Thailand. This research was funded by the Srina-kharinwirot University budget in the fiscal year 2551, under the Project agreement 151/2551 is acknowledged and for the consent to publish this paper.

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